• Benzimidazole carbamate residues in milk: Detection by Surface Plasmon Resonance-biosensor, using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method for extraction

      Keegan, Jemma; Whelan, Michelle; Danaher, Martin; Crooks, Steven; Sayers, Riona; Anastasio, Aniello; Elliott, C.; Brandon, David; Furey, A.; O'Kennedy, Richard (Elsevier, 2009-09-26)
      A surface plasmon resonance (SPR) biosensor screening assay was developed and validated to detect 11 benzimidazole carbamate (BZT) veterinary drug residues in milk. The polyclonal antibody used was raised in sheep against a methyl 5(6)-[(carboxypentyl)-thio]-2-benzimidazole carbamate protein conjugate. A sample preparation procedure was developed using a modified QuEChERS method. BZT residues were extracted from milk using liquid extraction/partition with a dispersive solid phase extraction clean-up step. The assay was validated in accordance with the performance criteria described in 2002/657/EC. The limit of detection of the assay was calculated from the analysis of 20 known negative milk samples to be 2.7 μg kg−1. The detection capability (CCβ) of the assay was determined to be 5 μg kg−1 for 11 benzimidazole residues and the mean recovery of analytes was in the range 81–116%. A comparison was made between the SPR-biosensor and UPLC–MS/MS analyses of milk samples (n = 26) taken from cows treated different benzimidazole products, demonstrating the SPR-biosensor assay to be fit for purpose.
    • Current trends in sample preparation for growth promoter and veterinary drug residue analysis

      Kinsella, Brian; O'Mahony, John; Malone, Edward; Moloney, Mary; Cantwell, Helen; Furey, A.; Danaher, Martin; Department of Agriculture, Food and the Marine, Ireland; 06RDTAFRC479; 07FHRITAFRC5 (Elsevier, 09/09/2009)
      A comprehensive review is presented on the current trends in sample preparation for isolation of veterinary drugs and growth promotors from foods. The objective of the review is to firstly give an overview of the sample preparation techniques that are applied in field. The review will focus on new techniques and technologies, which improve efficiency and coverage of residues. The underlying theme to the paper is the developments that have been made in multi-residue methods and particularly multi-class methods for residues of licensed animal health products, which have been developed in the last couple of years. The role of multi-class methods is discussed and how they can be accommodated in future residue surveillance.
    • Development and validation of a quantitative confirmatory method for 30 β-lactam antibiotics in bovine muscle using liquid chromatography coupled to tandem mass spectrometry

      Di Rocco, Melissa; Moloney, Mary; O’Beirne, T.; Earley, S.; Berendsen, B.; Furey, A.; Danaher, Martin; Department of Agriculture, Food and the Marine; 13/F484 (Elsevier BV, 2017-06)
      A method was developed for the confirmatory and quantitative analysis of 30 β-lactam antibiotic residues in bovine muscle. The method includes 12 penicillins (amoxicillin, ampicillin, cloxacillin, dicloxacillin, mecillinam, methicillin, nafcillin, oxacillin, penicillin G, penicillin V, piperacillin, ticarcillin), 12 cephalosporins (cefacetrile, cefadroxil, cephalexin, cefalonium, cefazolin, cefoperazone, cefotaxime, cefquinome, cefuroxime, desacetyl cephapirin, desfuroylceftiofur cysteine disulfide, desfuroylceftiofur dimer), five carbapenems (biapenem, doripenem, ertapenem, imipenem, meropenem) and faropenem. Samples were extracted using a simple solvent extraction with acetonitrile:water (80:20, v/v) and C18 dispersive solid-phase extraction (d-SPE) clean-up, followed by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) detection. Chromatography was performed on a reversed phase CSH C18 column, using a binary gradient separation comprising of 0.01% formic acid and 0.2 mM ammonium acetate in water (mobile phase A) and 0.01% formic acid in acetonitrile (mobile phase B). The mass spectrometer was operated in the positive electrospray ionisation mode (ESI(+)). Validation was performed following the 2002/657/EC guidelines. Trueness ranged between 69% and 143% and precision ranged between 2.0% and 29.9% under within-laboratory reproducibility conditions. The developed method uses minimal sample preparation and 30 test samples can be analysed by a single analyst in a single day. To the best of our knowledge, this is the first method for carbapenems in foodstuff that does not require derivatisation.
    • A dual validation approach to detect anthelmintic residues in bovine liver over an extended concentration range

      Kinsella, Brian; Whelan, Michelle; Cantwell, Helen; McCormack, Martin; Furey, A.; Lehotay, Stephen J.; Danaher, Martin; Department of Agriculture, Food and the Marine, Ireland; European Union; 06RDTAAFRC479; et al. (Elsevier, 21/08/2010)
      This paper describes a method for the detection and quantification of 38 residues of the most widely used anthelmintics (including 26 veterinary drugs belonging to the benzimidazole, macrocyclic lactone and flukicide classes) in bovine liver using two different protocols for MRL and non-MRL levels. A dual validation approach was adopted to reliably quantify anthelmintic residues over an extended concentration range (1–3000 gkg−1). Sample extraction and purification was carried out using a modified QuEChERS method. A concentration step was included when analysing in the low gkg−1 range. Rapid analysis was carried out by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS), which was capable of detecting residues to <2 gkg−1. The method has been single-laboratory validated according to the 2002/657/EC guidelines and met acceptability criteria in all but a few cases. The inclusion of 19 internal standards, including 14 isotopically labelled internal standards, improved accuracy, precision, decision limit (CC˛) and detection capability (CCˇ).
    • Protocols and strategies to study the migration of veterinary drug residues into milk and dairy products in licensed trials

      Power, C.; Sayers, Riona; O'Brien, Bernadette; Furey, A.; Danaher, Martin; Jordan, Kieran (Teagasc (Agriculture and Food Development Authority), Ireland, 2013)
      In the interest of animal welfare, and in order that the results from animal trials are considered valid for inclusion in the development of regulations, it is necessary that such trials are undertaken in accordance with the appropriate licensing arrangements. In January 2013, new licensing arrangements were introduced in the European Union. The aim of this paper is to outline the legislative strategy required for obtaining licences for animal trials and based on live animal trials with flukicides, establishes a blueprint for obtaining the appropriate licences and undertaking the experiments.
    • Protocols and strategies to study the migration of veterinary drug residues into milk and dairy products in licensed trials – Corrigendum

      Power, C.; Sayers, Riona; O'Brien, Bernadette; Furey, A.; Danaher, Martin; Jordan, Kieran (Teagasc (Agriculture and Food Development Authority), Ireland, 2014)
      Corrigendum
    • Review of studies on flukicide residues in cows’ milk and their transfer to dairy products

      Power, C.; Sayers, Riona; O'Brien, Bernadette; Furey, A.; Danaher, Martin; Kieran, Jordan; Teagasc Walsh Fellowship Programme (Teagasc (Agriculture and Food Development Authority), Ireland, 2013)
      Flukicides are widely used to treat infestations of liver fluke in dairy cattle. This could result in flukicide residues in milk if animals are improperly treated or if withdrawal periods are not properly observed. The purpose of this review is to summarise the results of studies on depletion of flukicides from milk and the transfer of flukicide residues to dairy products, if present in the milk. As the depletion of flukicide residues from milk of animals treated during lactation was relatively slow, the studies support the view that the dry period (when milk is not being used for human consumption) is the most suitable time for flukicide treatment. Migration of residues to product occurred at different rates, depending on the drug in question. Generally, concentration of flukicides occurred in cheese, butter and skim milk powder. Pasteurisation or heat treatment during spray drying had no impact in reducing residues.